CN105197928A - Method for preparing high surface area activated carbons - Google Patents
Method for preparing high surface area activated carbons Download PDFInfo
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- CN105197928A CN105197928A CN201510639434.0A CN201510639434A CN105197928A CN 105197928 A CN105197928 A CN 105197928A CN 201510639434 A CN201510639434 A CN 201510639434A CN 105197928 A CN105197928 A CN 105197928A
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- surface area
- specific surface
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- active carbon
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Abstract
The invention discloses a method for preparing high surface area activated carbons, wherein carbon precursors are soaked into a preparation liquid firstly, are filtered to obtain a mixture 1 after being soaked by heating, then the mixture 1 is dried to obtain a solid substance, then the solid substance is added into a mixture of carbonic acids and glycidyl methacrylate, is heated to 150-200 DEG C for 10-20mins by being protected through inert gases after being stirred in a vacuum condition, then is cooled to the room temperature to obtain an intermediate 1, the intermediate 1 is heated to 800-900 DEG C for 120-180mins in a hydrogen atmosphere at last, then is mutually cooled to the room temperature, and then is cleaned and dried to obtain activated carbons. The activated carbons which are prepared through the method for preparing the high surface area activated carbons have excellent surface area and adsorptive property.
Description
Technical field
The invention belongs to gac preparing technical field, be specifically related to a kind of preparation method of active carbon with high specific surface area.
Background technology
Gac is with fat coal, wood chip or shell for raw material, through a kind of porousness charcoal element material that the technological processs such as machine-shaping, charing, activation are made.It has certain physical strength, very large specific surface area and extremely strong absorption property.Energy decolouring, deodorization, desulfurization, de-benzene, optionally can also remove some impurity atom and mechanical impurity in liquid phase or gas phase.Also can adsorb some catalyzer, chemical reaction velocity is accelerated greatly, be good support of the catalyst.Therefore gac has purposes widely in all respects of national defence, chemical industry, oil, weaving, food, medicine, nuclear industry, urban construction, environment protection and human lives.Granular carbon performance and purposes.Active carbon with high specific surface area is in the large-scale production eighties in last century, and its performance is significantly better than conventional gac, but the general specific surface area of active carbon with high specific surface area conventional is at present at 3000m
2within/g, absorption property is also limited simultaneously.Along with the development of industry, in some occasion as its performance of the storage request of hydrogen especially specific surface area still needs further lifting.
Summary of the invention
The object of the invention is to the preparation method that a kind of active carbon with high specific surface area is provided to overcome above the deficiencies in the prior art, improving specific surface area and the absorption property of gac.
Technical scheme of the present invention is as follows:
A preparation method for active carbon with high specific surface area, comprises the following steps:
Step one, will be dipped in containing carbon matrix precursor and prepare, in liquid, to be warming up to 40-45 DEG C, and soak 150-200 minute, filter, obtain mixture one, wherein prepare the mixed solution that liquid is MALEIC ANHYDRIDE, volatile salt and water;
Step 2, dries mixture one, obtains solids;
Step 3, gets solids and joins in the mixture of carbonic acid and glycidyl methacrylate, stirs 50-100 minute under vacuum, then under the condition of protection of inert gas, 150-200 DEG C is warming up to, keep 10-20 minute, be then down to room temperature, obtain intermediate one;
Step 4, is heated to 800-900 DEG C by intermediate one in atmosphere of hydrogen, keeps 120-180 minute, is then naturally down to room temperature, then by cleaning, drying, obtains gac.
The preparation method of described active carbon with high specific surface area, containing carbon matrix precursor in step one is refinery coke, coal or agricultural crop straw.
The preparation method of described active carbon with high specific surface area, the mass ratio that step one prepares MALEIC ANHYDRIDE in liquid, volatile salt and water is 1:0.6-2:15-20.
The preparation method of described active carbon with high specific surface area, in step 2, bake out temperature is 80-100 DEG C.
The preparation method of described active carbon with high specific surface area, in step 3, the mass ratio of solids, carbonic acid and glycidyl methacrylate is 1:2-4:0.5-1.
The preparation method of described active carbon with high specific surface area, in step 3, rare gas element is nitrogen.
The preparation method of described active carbon with high specific surface area, in step 3, the vacuum tightness of vacuum condition is 0.005-0.01MPa.
The gac that preparation method provided by the invention prepares has good performance, and wherein specific surface area reaches 4120m
2/ more than g, ash content reaches within 3.4%, and iodine sorption value reaches 1256mg/g, and Penetrating curve reaches more than 1325mg/g, has excellent specific surface area and absorption property.
Embodiment:
Embodiment 1
A preparation method for active carbon with high specific surface area, comprises the following steps:
Step one, is dipped in 300g refinery coke and prepares, in liquid, to be warming up to 40-45 DEG C, soak 150-200 minute, filter, obtain mixture one, wherein prepare the mixed solution that liquid is 60g MALEIC ANHYDRIDE, 36g volatile salt and 900g water;
Step 2, dries mixture one, and bake out temperature is 80 DEG C, obtains solids;
Step 3, getting 200g solids joins in the mixture of 400g carbonic acid and 100g glycidyl methacrylate, be stir 50 minutes under the vacuum condition of 0.005MPa in vacuum tightness, then under the condition of nitrogen protection, 150 DEG C are warming up to, keep 10 minutes, then be down to room temperature, obtain intermediate one;
Step 4, is heated to 800 DEG C by intermediate one in atmosphere of hydrogen, keeps 120 minutes, is then naturally down to room temperature, then by cleaning, drying, obtains gac.
Embodiment 2
A preparation method for active carbon with high specific surface area, comprises the following steps:
Step one, is dipped in 400g coal and prepares, in liquid, to be warming up to 42 DEG C, to soak 170 minutes, filter, obtain mixture one, wherein prepare the mixed solution that liquid is 60g MALEIC ANHYDRIDE, 60g volatile salt and 1080g water;
Step 2, dries mixture one, and bake out temperature is 85 DEG C, obtains solids;
Step 3, getting solid 400g thing joins in the mixture of 1200g carbonic acid and 240g glycidyl methacrylate, be stir 70 minutes under the vacuum condition of 0.006MPa in vacuum tightness, then under the condition of argon shield, 160 DEG C are warming up to, keep 15 minutes, then be down to room temperature, obtain intermediate one;
Step 4, is heated to 850 DEG C by intermediate one in atmosphere of hydrogen, keeps 150 minutes, is then naturally down to room temperature, then by cleaning, drying, obtains gac.
Embodiment 3
A preparation method for active carbon with high specific surface area, comprises the following steps:
Step one, is dipped in agricultural crop straw 500g and prepares, in liquid, to be warming up to 44 DEG C, to soak 180 minutes, filter, obtain mixture one, wherein prepare the mixed solution that liquid is 80g MALEIC ANHYDRIDE, 130g volatile salt and 1500g water;
Step 2, dries mixture one, and bake out temperature is 90 DEG C, obtains solids;
Step 3, getting 500g solids joins in the mixture of 1500g carbonic acid and 400g glycidyl methacrylate, be stir 80 minutes under the vacuum condition of 0.006MPa in vacuum tightness, then under the condition of nitrogen protection, 190 DEG C are warming up to, keep 18 minutes, then be down to room temperature, obtain intermediate one;
Step 4, is heated to 880 DEG C by intermediate one in atmosphere of hydrogen, keeps 170 minutes, is then naturally down to room temperature, then by cleaning, drying, obtains gac.
Embodiment 4
A preparation method for active carbon with high specific surface area, comprises the following steps:
Step one, is dipped in agricultural crop straw 400g and prepares, in liquid, to be warming up to 45 DEG C, to soak 200 minutes, filter, obtain mixture one, wherein prepare the mixed solution that liquid is 80g MALEIC ANHYDRIDE, 160g volatile salt and 1600g water;
Step 2, dries mixture one, and bake out temperature is 100 DEG C, obtains solids;
Step 3, getting solids 400g joins in the mixture of 1600g carbonic acid and 400g glycidyl methacrylate, be stir 100 minutes under the vacuum condition of 0.01 in vacuum tightness, then under the condition of nitrogen protection, 200 DEG C are warming up to, keep 20 minutes, then be down to room temperature, obtain intermediate one;
Step 4, is heated to 900 DEG C by intermediate one in atmosphere of hydrogen, keeps 180 minutes, is then naturally down to room temperature, then by cleaning, drying, obtains gac.
Reference examples
A preparation method for active carbon with high specific surface area, comprises the following steps:
Step one, will mix agricultural crop straw and dry, bake out temperature is 90 DEG C, obtains solids;
Step 2, getting 500g solids joins in the mixture of 1500g carbonic acid and 400g glycidyl methacrylate, be stir 80 minutes under the vacuum condition of 0.006MPa in vacuum tightness, then under the condition of nitrogen protection, 190 DEG C are warming up to, keep 18 minutes, then be down to room temperature, obtain intermediate one;
Step 3, is heated to 880 DEG C by intermediate one in atmosphere of hydrogen, keeps 170 minutes, is then naturally down to room temperature, then by cleaning, drying, obtains gac.
Carry out performance test to the gac that above embodiment prepares, result is as follows:
| Project | Specific surface area/m2/g | Ash content/% | Iodine sorption value/mg/g | Penetrating curve/mg/g |
| Embodiment 1 | 4120 | 3.2 | 1256 | 1325 |
| Embodiment 2 | 4250 | 3.2 | 1315 | 1423 |
| Embodiment 3 | 4536 | 3.1 | 1387 | 1489 |
| Embodiment 4 | 4453 | 3.3 | 1358 | 1453 |
| Reference examples | 3130 | 3.4 | 852 | 945 |
As can be seen from the above results, the gac that preparation method provided by the invention prepares has good performance, and wherein specific surface area reaches 4120m
2/ more than g, ash content reaches within 3.4%, and iodine sorption value reaches 1256mg/g, and Penetrating curve reaches more than 1325mg/g, therefore has excellent specific surface area and absorption property.Reference examples is the further test carried out on the basis of embodiment 3, immersion process in wherein carry out step one, other are identical with embodiment 3, result can be found out, the gac specific surface area finally obtained and adsorptive value have obvious decline, therefore can illustrate, the immersion process in preparation method provided by the invention in step one can significantly improve specific surface area and the absorption property of material.
Claims (7)
1. a preparation method for active carbon with high specific surface area, is characterized in that, comprises the following steps:
Step one, will be dipped in containing carbon matrix precursor and prepare, in liquid, to be warming up to 40-45 DEG C, and soak 150-200 minute, filter, obtain mixture one, wherein prepare the mixed solution that liquid is MALEIC ANHYDRIDE, volatile salt and water;
Step 2, dries mixture one, obtains solids;
Step 3, gets solids and joins in the mixture of carbonic acid and glycidyl methacrylate, stirs 50-100 minute under vacuum, then under the condition of protection of inert gas, 150-200 DEG C is warming up to, keep 10-20 minute, be then down to room temperature, obtain intermediate one;
Step 4, is heated to 800-900 DEG C by intermediate one in atmosphere of hydrogen, keeps 120-180 minute, is then naturally down to room temperature, then by cleaning, drying, obtains gac.
2. the preparation method of active carbon with high specific surface area according to claim 1, is characterized in that, containing carbon matrix precursor in step one is refinery coke, coal or agricultural crop straw.
3. the preparation method of active carbon with high specific surface area according to claim 1, is characterized in that, the mass ratio that step one prepares MALEIC ANHYDRIDE in liquid, volatile salt and water is 1:0.6-2:15-20.
4. the preparation method of active carbon with high specific surface area according to claim 1, is characterized in that, in step 2, bake out temperature is 80-100 DEG C.
5. the preparation method of active carbon with high specific surface area according to claim 1, is characterized in that, in step 3, the mass ratio of solids, carbonic acid and glycidyl methacrylate is 1:2-4:0.5-1.
6. the preparation method of active carbon with high specific surface area according to claim 1, is characterized in that, in step 3, rare gas element is nitrogen.
7. the preparation method of active carbon with high specific surface area according to claim 1, is characterized in that, in step 3, the vacuum tightness of vacuum condition is 0.005-0.01MPa.
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| CN201510639434.0A CN105197928A (en) | 2015-09-30 | 2015-09-30 | Method for preparing high surface area activated carbons |
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| CN201510639434.0A CN105197928A (en) | 2015-09-30 | 2015-09-30 | Method for preparing high surface area activated carbons |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800296A (en) * | 2016-12-23 | 2017-06-06 | 镇江华域环保设备制造有限公司 | A kind of preparation method of purification of air active carbon with high specific surface area |
| CN106986337A (en) * | 2016-12-23 | 2017-07-28 | 镇江华域环保设备制造有限公司 | A kind of preparation method of air cleaning porous activated carbon |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456555A (en) * | 2008-09-04 | 2009-06-17 | 南昌大学 | Method for preparing high mode number waterglass and active carbon by rice hull ash |
| CN104003387A (en) * | 2014-06-10 | 2014-08-27 | 厦门大学 | Method for preparing active carbon by taking biomass pyrolytic carbon as raw material |
-
2015
- 2015-09-30 CN CN201510639434.0A patent/CN105197928A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456555A (en) * | 2008-09-04 | 2009-06-17 | 南昌大学 | Method for preparing high mode number waterglass and active carbon by rice hull ash |
| CN104003387A (en) * | 2014-06-10 | 2014-08-27 | 厦门大学 | Method for preparing active carbon by taking biomass pyrolytic carbon as raw material |
Non-Patent Citations (3)
| Title |
|---|
| STAVROPOULOS G G ET: "《Precursor materials suitability for super activated carbons production》", 《FUEL PROCESSING TECHNOLOGY》 * |
| 何东平等: "《油脂工厂设计手册•下册》", 31 August 2012 * |
| 姜瑞霞等: "《高温氢气处理对活性炭及钯炭催化剂性能的影响》", 《化学反应工程与工艺》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800296A (en) * | 2016-12-23 | 2017-06-06 | 镇江华域环保设备制造有限公司 | A kind of preparation method of purification of air active carbon with high specific surface area |
| CN106986337A (en) * | 2016-12-23 | 2017-07-28 | 镇江华域环保设备制造有限公司 | A kind of preparation method of air cleaning porous activated carbon |
| CN106800296B (en) * | 2016-12-23 | 2019-03-29 | 镇江华域环保设备制造有限公司 | A kind of preparation method of air cleaning active carbon with high specific surface area |
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Application publication date: 20151230 |